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EP1317886B1 - Use of micronised zeolites as filter material - Google Patents

Use of micronised zeolites as filter material Download PDF

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Publication number
EP1317886B1
EP1317886B1 EP02090411A EP02090411A EP1317886B1 EP 1317886 B1 EP1317886 B1 EP 1317886B1 EP 02090411 A EP02090411 A EP 02090411A EP 02090411 A EP02090411 A EP 02090411A EP 1317886 B1 EP1317886 B1 EP 1317886B1
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EP
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Prior art keywords
fan blades
filter
micronized
zeolites
zeolite
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German (de)
French (fr)
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EP1317886A1 (en
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Tihomir Lelas
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Priority to SI9930982T priority Critical patent/SI1317886T1/en
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12Powders or granules
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/06Aluminium; Calcium; Magnesium; Compounds thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16Inorganic salts, minerals or trace elements
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/16Use of materials for tobacco smoke filters of inorganic materials
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/16Use of materials for tobacco smoke filters of inorganic materials
    • A24D3/166Silicic acid or silicates
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/06Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
    • A61K33/08Oxides; Hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C13/00Disintegrating by mills having rotary beater elements ; Hammer mills
    • B02C13/20Disintegrating by mills having rotary beater elements ; Hammer mills with two or more co-operating rotors
    • B02C13/205Disintegrating by mills having rotary beater elements ; Hammer mills with two or more co-operating rotors arranged concentrically
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/026After-treatment
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/0076Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials characterised by the grain distribution
    • C04B20/008Micro- or nanosized fillers, e.g. micronised fillers with particle size smaller than that of the hydraulic binder
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/18Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12HPASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/02Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
    • C12H1/04Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material
    • C12H1/0408Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of inorganic added material
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/60Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

Definitions

  • the invention relates to the use of micronized zeolites as filter cloth.
  • a device which can crush zeolites so that their effectiveness is improved is already out of DE 197 55 921.2 known.
  • the invention there describes a method for improving the effectiveness of active ingredients, which consist of at least mineral substances, by subjecting these active ingredients to tribomechanical activation, in which the surface of the treated active ingredients is increased and the structure of which is destabilized to increase the chemical potential.
  • the activation of the minerals is done by intervening in the integrity of the crystal lattice, resulting in a kind of damage, which in turn in the form of an activation, for example, electrical type, noticeable.
  • the DE 197 55 921.2 regards as advantageous the treatment of zeolites, which are described there for the salutary consumption for humans; Also calcites for the agricultural sector are mentioned that by the from the DE 197 55 921.2 known device to be achieved micronization is 20 microns per particle, with only about 78% of all particles reached this magnitude.
  • the EP 0 740 907 A describes like that US 3,327,718 A and the US 4,038,992 A the use of zeolite mineral in cigarette filters.
  • micronized zeolites are used with a particle size diameter of less than 0.5 microns as filter cloth, which consist of rotors consisting of discs on which the fan blades on one side are arranged and wherein the fan blades are connected to the rings and pass through in corresponding channels on the respective opposite rotor disc, which prevent a passage of material under the Ventitatorschaufeh.
  • the novel device causes diverse chemical and chemical-physical changes in mineral raw material components.
  • the effects created by dynamic friction processes give these minerals new properties that can be used technologically and commercially in the manufacture of diverse products.
  • the mineral heulandite / clinoptylolite has been found advantageous by virtue of its properties, namely its ability to absorb water, its selectivity and ion exchange capacity, and its chemical composition, which has shown that this mineral is absolutely harmless to human consumption.
  • the calcium content of this mineral indicates that it is a calcium zeolite formed in a tuff-like structure, ie, it is a kind of the mineral clinoptilolite having the properties of the heulandite group.
  • the measured volume weight of the studied mineral clinoptiloite ranges from 1.41 to 1.43 g / cm 3 .
  • Difractometric and thermo-gravimetric studies showed that approximately the same zeolite content exists in all the samples studied.
  • the results of the X-ray studies show the presence of the following types of minerals: heulandithe (clinoptilolites), and subsequently essentially quartz, sand, plagioclase and, in a small amount, also biothythe.
  • the loss on ignition is: ⁇ u> Table 2 ⁇ / u> Loss on ignition [wt .-%] H 2 O at 100 ° C 3.34 to 3.36 H 2 O at 300 ° C 5.42 to 5.51 H 2 O at 500 ° C 2.60 to 2.64 H 2 O at 1000 ° C 2.50 to 2.51 All in all 13.86 to 13.92
  • the following table shows examples of conductivity and pH measurements of the suspension in untreated and treated zeolites: ⁇ u> Table 4 ⁇ / u> Mixing time of the suspension a Concentration of zeolite (mg / ml H 2 O) pH b (unactivated zeolite) pH b (zeolite treated according to the invention) Conductivity c (unactivated zeolite) ⁇ S / cm Conductivity c (zeolite treated according to the invention) ⁇ S / cm 2 hours. 20 7.35 7.48 157 147 2 hours. 40 6.45 7.22 198 180 2 hours.
  • the result is that the pH of the untreated to the treated zeolites increases while the conductivity decreases.
  • the material treated according to the invention shows surprising effects with regard to the minimization of harmful components of filter cigarettes.
  • the classic filter is the cellulose acetate filter.
  • additives such as activated carbon, zeolites, silica gel, magnesium silicate and artificial hemoglobin are used.
  • the material treated according to the invention surprisingly increases the efficiency and selection of the filters, as well as stopping and improving the desired taste of the cigarette; while the suction resistance of the filter is hardly changed.
  • the treated zeolites have a larger Absorption strength, which is due to the changes in the crystal lattice.
  • a filter additive in cellulose acetate filters has proven to be a powder with a particle size of 0.2 to 0.5 microns.
  • the zeolites treated according to the invention can be applied directly to the cellulose acetate fiber or the paper or crest - such as an additive in the cavity of a multifilter, combined with the dual filter, etc.
  • Filters that were the subject of a controlled experiment were produced by adding zeolites treated according to the invention directly to the cellulose acetate fiber after using plasticizers (triacetin) prior to forming the filter rods in the cylinder.
  • the powder was applied directly to the fiber through a specially designed dosimeter. This made it possible to add almost uniformly up to 70 mg of the zeolite treated according to the invention per filter rod.
  • This way of adding the powder does not significantly affect the work of the conventional machines and the forming of the filter sticks, since the machines for making the sticks have a dedicated space in the working flow for this application.
  • the technology of rod production does not change significantly. The technological process is only increased by the price of the additives.
  • the results obtained are averages of the measurements of 500 filter rods from each sample.
  • the proportion of the treated zeolite added was calculated from 525 ° C due to the difference in the amount of ash obtained when burning the filter sticks in the Mufon oven.
  • For the processing of the cigarette was substantially conventional filter paper without ventilation and a mixture of tobacco, which is used in the production of full flavor American Blend cigarettes.
  • the processed cigarettes were sorted by weight and suction resistance and tested on the smoking machine (Borgwaldt RM 20) according to the ISO standard. Each sample was tested 5 times on the machine.
  • the amount of Total Particulate Matter, nicotine, CO 2 , water and tar were determined. All analyzes were performed according to the current ISO standard; the amount of nicotine in the dry smoke condensate was carried out by extraction with 2-propanol and subsequent HPLC.
  • samples 5 - 11.3 mg and sample 4 - 1.66 mg have an improved smoky taste and a pronounced aroma, so that they are generally more agreeable are smoking.
  • the following table shows the measured average values of the filters after smoking.
  • the amount of dry smoke condensate was calculated from the difference in the amount of production material before and after smoking.
  • the amount of nicotine was determined by extraction from the filter in 2-propanol and water by the Karl-Fisher method.
  • the results show that the filters applied with the zeolite treated according to the invention have an increased ability to absorb of dry smoke condensate, nicotine, and water, which underlines the previous measurements and results.
  • the application of the zeolite treated according to the invention to cellulose acetate fiber of cigarette filters thus leads to an increased retention of harmful components of the main stream of the cigarette smoke, satisfactory physical properties, but without having a negative effect on the degustative and smoking properties of a cigarette.
  • the addition of 0.50 mg of the zeolite treated per filter according to the invention eliminates 4% dry smoke condensate, CO 2 and nicotine, and 11% water.
  • An addition of 11.30 mg of zeolite per filter treated according to the invention eliminates 27% dry smoke condensate, CO 2 and nicotine, and 42% water from the main stream of smoke.
  • selenium up to 25 .mu.g / filter
  • selenium up to 25 .mu.g / filter
  • FIG. 1 shows a device 10 for the fine grinding and micronization, and the homogenization of various solid and liquid raw material components.
  • the principle is such that the starting material is sucked through the center of the rotors into the processing space of the device. The entry is favored by the action of centrifugal forces in the space between the fan blades and is accelerated due to the prevailing air currents there; so that the material collides with the already processed material.
  • the source material changes direction of movement in very short intervals; As a result, it is crushed and micronized.
  • the device 10 consists of a hinged housing 11 with a Materialeinfarschacht 11d, in which there are two rotor discs 12, which are opposed to each other and operated by respective motors 13 via belt 13a in opposite directions, so that they rotate at the same angular velocity.
  • the housing 11 and the motors 13 are mounted on the foundation 14 and form an independent unit.
  • FIG 2 shows that the housing 11 is constructed of two parts: a housing side 11 a for the material import and a further housing side 11 b with insertion shaft 11 c. These two sides 11a, 11b are bolted together. On both sides of the housing 11 are the carrier 15, in which the bearings 16 and stretch rods 17 are installed. On the side 11a for the material import is a pipe 18 for the controlled import of the material; on the lower side there is an opening 19 for the discharge of the finished material.
  • Figures 3, 4 and 5 show that on the rotor disks 12 a plurality of concentric rings 20 are arranged with the pins 21 and fan blades 22, which are constructed and oriented so that they can run past each other without contact as they rotate in opposite directions - indicated by the Turning 25. Minimum two wreaths are required which are driven by the two rotors.
  • the task of the striker pins 21 and fan blades 22 is to create turbulent airflows for the acceleration of the processed material so that shocks and friction among the granules at certain angles will create dynamic conditions.
  • the channels 23 on the discs prevent the passage of material under the fan blades 22, see. Figure 3 a and 3b.
  • the starting granules (not shown), introduced by the central portion 18 of the engine system by suction, accelerated by the air streams 26 and controlled so that the grains collide with each other due to repeated movement direction and rub against each other in very short time intervals.
  • the tools and other parts of the device do not touch or only slightly - but it comes in no case to destruction of the tools.
  • An interaction occurs among the granules to such an extent that in the granules the internal energy is exchanged since the collisions are aplastic (see Figures 4 and 5).
  • the material which has been finely ground and micronized by the device according to the invention shows increased free energy and reactivity.
  • the innovation is therefore in the design (shape, toothing, inclination) and interchangeability of pins and fan blades on the constructed channels, which are located on the rotor disc, as well as in the selection of material for the development of fan blades.
  • the rotation discs of the device rotate at the same angular velocity, but move in opposite directions.
  • the raw material is introduced into the central portion of the rotating disk through the suction pipe 18, and due to centrifugal forces, the granules of the raw material component are accelerated toward the outer periphery of the casing.
  • the granules strike the rims 20 of the fan blades 22, which rotate in the opposite direction. They change the direction of movement due to the change of direction of the fan blades.
  • the grains beat and rub one against the other, then proceeding into another ring 20 with fan blades 22, again changing the direction of movement in accordance with the directional change of the rotating disk until they leave the paddle system.
  • the granules strike the wall of the housing and are transported away through the outlet opening 19.
  • FIGS. 3a and 3b show that the channels 23 on the disks 12, in which the fan blades 22 pass, prevent the material passage under the fan blades 22.
  • Their shape is defined according to the properties of the respective raw material components (material) to be processed - ie granulation of the starting material, its moisture, hardness, origin, chemical composition and the like. If z. For example, if the input granulation of the material is ⁇ 1 mm, this means that the minimum distance between the fan blades and the channels on the Slices should be greater than 1 mm, to allow even the passage of the material.
  • the fan blades are occupied due to their shape, inclination and toothing in the process of fine grinding and micronization with a fine layer of the processed material and are protected in this way from the impact and friction effect of the input material.
  • the wear of the surface of the fan blades is thus minimized and the life extended significantly. Further, the energetic charge of the material being treated is raised when the granules collide with each other and not with the parts of the fan blades.
  • the technological parameters such as the number of fan blades, their inclination, the shape of the blade teeth, number of fan crowns, angular velocity of the discs, define the later properties of the processed material.
  • FIG. 3b further disc channels (23) are shown in more detail.
  • recesses (20a see Figures 3a, 3b) are located at those locations corresponding to the row of corrugations (20) of the opposite rotor (13), within which the fan blades (22) of the opposite ring (20). 20).
  • the channels (23) cover each other with the length a, which is 2 - 5 mm. They form a kind of labyrinth, which prevents the passage of the material under the fan blades. The emergence of the labyrinth increases resistance to the flow under the fan blades. Thus, it is achieved that the granules of the starting material move through the main flow between the fan blades.
  • the shape of the channels is in accordance with technical-technological characteristics of the raw material components of processed material (granulation of the starting material, its moisture, hardness, origin, chemical composition and the like). If there were not the disc channels, the source material would move due to the centrifugal forces passing from the center to the periphery of the discs on the fan blades and disc. At the initial granulation of the material of 0-1 mm, the distance between the fan blades and the channels must be greater than 1 mm to allow passage of the material at all, advantageously a distance of 2 mm has proven to be the same as for the occlusion a.
  • Figures 6, 6a, 6b and 6c show the geometry of the fan blades 22 and the pins 21.
  • the rim 20, the fan blades 22 and the pins 21 are made of high carbon steel.
  • An alternative is to make the porcelain pin and the fan blades made of steel.
  • the degree of flexing of the fan blades is defined by the ratio of lengths a and b, where b represents 10% of the chord length.
  • the arrangement of the fan blades is fixed.
  • the shape of the fan blades, profiled collision surface 22a, 22b and the incline secure the filling of the fan blades with the starting material and are thus protected from the wear effect of the starting material, which acts to extend the life of the fan blades.
  • the teeth 22b on the fan blades hold the first layer of starting material on the collision surface 22a while the second layer slowly slips over the first layer and this second layer accepts the impacts of the incoming source material.
  • the pin 21 is pressed into the rotor disk 12.
  • the symmetry axis of the pen 21 is located in the axis of symmetry of the degree of bending of the fan blades 22, so that the geometry of the system of fan blades / pins is optimally achieved.
  • the granules strike the end face of the fan blades, and in particular onto and into the pins.
  • the pen is thus worn.
  • the pin is replaced by pressing or drilling through a new one.
  • the problem of the vibrations and the strength of the pins is solved in that the pin 21 with the area of 1/3 of his. StiftFoodes to a corresponding recess of the fan blade 22 to these fan blades "leans", and does not lean against the fan blades on a straight surface.
  • the fan blades 22 are deformed by cold pressing or by forging, whereby the forging serves for better curing.
  • segment fan blades (FIGS. 7, 7a).
  • the segment fan blades 22 are made of ceramic or cast steel.
  • the channels are incorporated into the rotor discs 12, in which the segment fan blades are placed with indefinite deposits.
  • the accuracy of the settings and the strength of the fan blades is determined by the profile of the channels and by the friction between the segment fan blades and the supporting disc.
  • the classification of the teeth 22b and their size is Depending on the length of the fan blades 22, angle ⁇ is 30 ° - 120 °, and angle ⁇ is 60 ° - 120 °.
  • the degree of flexing of the fan blades is defined by the ratio of lengths a and b, where b represents 10% of the chord length.
  • the shape of the fan blades, the profiled (toothed) collision surface and the slope ensure that the fan blades are filled with the source material and thus protected from the wear effect of the source material, which acts to extend the life of the fan blades.
  • the teeth 22b on the fan blades, as in FIG. 6, hold the first layer of the starting material on the collision surface 22a, while the second layer slowly slips over the first layer, and this second layer absorbs the impacts of the incoming source material.
  • This embodiment has the advantage over the previous embodiment ( Figure 6) that the fan blades can be installed with different inclinations (angle ⁇ ); Thus, the replacement of the fan blades is easier.
  • the shape of the fan blades has no recess for the pins.

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  • Chemical & Material Sciences (AREA)
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  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The two rotors comprise discs (12) with fan blades attached on one side. The fan blades are arranged in concentric rings received by corresponding channels in the opposing rotor disc in order to prevent passage of material under the blades. <??>The machine consists of a casing with two rotors, each of which comprises several rings that engage inside one another and are driven in counter-rotation with an identical angular velocity. The rings are separately controlled and carry a number of fan blades on both of the ring walls, acting as a collision barrier for the material being milled and micronized. Centrifugal force carries the material from the inner ring towards the outer ring. <??>Independent claims are also included for (a) the use of micronized zeolite as a drug for treating cancer, metabolism, heart and blood circulation complaints, multiple sclerosis and rheumatism, as a drug for dermatological applications, as a cosmetic, as an additive for bakery and confectionery products, as a filter material, as a filter additive for filter cigarettes, and as an additive for tile making, (b) the use of micronized minerals, especially calcites, as plant protection agents, (c) the use of micronized minerals, especially calcites, dolomites and carbonates, as fertilizers and/or yield increasing agents in agriculture, (d) the use of micronized minerals as odor reducing agents, and (e) the use of micronized clay components for reducing the sintering temperature during sintering processes used in the ceramic or glass industry.

Description

Die Erfindung betrifft die Verwendung mikronisierter Zeolithe als Filterstoff.The invention relates to the use of micronized zeolites as filter cloth.

Eine Vorrichtung, welche Zeolithe derart zerkleinern kann, dass deren Wirksamkeit verbessert wird, ist bereits aus der DE 197 55 921.2 bekannt. Die dortige Erfindung beschreibt ein Verfahren zur Verbesserung der Wirksamkeit von Wirkstoffen, die mindestens aus Mineralstoffen bestehen, indem diese Wirkstoffe einer tribomechanischen Aktivierung unterzogen werden, bei der die Oberfläche der behandelten Wirkstoffe vergrößert und deren Struktur zur Vergrößerung des chemischen Potentials destabilisiert wird. Die Aktivierung der Mineralstoffe geschieht dadurch, dass in die Integrität der Kristallgitter eingegriffen wird, wodurch sich eine Art Beschädigung ergibt, die sich wiederum in Form einer Aktivierung, beispielsweise auch elektrischer Art, bemerkbar macht. Die DE 197 55 921.2 sieht dabei als vorteilhaft die Behandlung von Zeolithen an, die dort zum heilsamen Verzehr für Menschen beschrieben werden; auch Calcite für den Agrarbereich werden erwähntdassDie durch die aus der DE 197 55 921.2 bekannte Vorrichtung zu erzielende Mikronisierung liegt bei 20 µm pro Teilchen, wobei nur ca. 78 % aller Teilchen diese Größenordnung erreichten.A device which can crush zeolites so that their effectiveness is improved, is already out of DE 197 55 921.2 known. The invention there describes a method for improving the effectiveness of active ingredients, which consist of at least mineral substances, by subjecting these active ingredients to tribomechanical activation, in which the surface of the treated active ingredients is increased and the structure of which is destabilized to increase the chemical potential. The activation of the minerals is done by intervening in the integrity of the crystal lattice, resulting in a kind of damage, which in turn in the form of an activation, for example, electrical type, noticeable. The DE 197 55 921.2 regards as advantageous the treatment of zeolites, which are described there for the salutary consumption for humans; Also calcites for the agricultural sector are mentioned that by the from the DE 197 55 921.2 known device to be achieved micronization is 20 microns per particle, with only about 78% of all particles reached this magnitude.

Aus der US 5,723,397 A und der US 5,871,650 wird die Verwendung von Zeolithen in Membran oder Filtern offenbart. Dabei werden auch Zeolithe mit einem Korngrößendurchmesser von weniger als 0,5 µm verwendet. Eine Aktivierung der Zeolithe durch einen speziellen Zerkleinerungsprozess wird in beiden Dokumenten jedoch nicht offenbart.From the US 5,723,397 A and the US 5,871,650 discloses the use of zeolites in membrane or filters. Here are also zeolites with a grain size diameter of less than 0.5 microns used. Activation of the zeolites by a special comminution process is not disclosed in either document.

Die EP 0 740 907 A beschreibt wie die US 3,327,718 A und die US 4,038,992 A die Verwendung von Zeolithmineral in Zigarettenfiltern.The EP 0 740 907 A describes like that US 3,327,718 A and the US 4,038,992 A the use of zeolite mineral in cigarette filters.

Ausgehend von diesem Stand der Technik ist es daher Aufgabe der vorliegenden Erfindung, hochaktive Zeolithe zur Verwendung als Filterstoff zur Verfügung zu stellen, insbesondere für Zigarettenfilter.Based on this prior art, it is therefore an object of the present invention to provide highly active zeolites for use as a filter cloth, in particular for cigarette filters.

Gelöst wird diese Aufgabe durch die im Patentanspruch 1 und 2 aufgeführten Merkmale, nämlich dadurch, dass mikroniserte Zeolithe mit einem Korngrößendurchmesser von weniger als 0,5 µm als Filterstoff verwendet werden, welche durch Rotoren, die aus Scheiben bestehen, auf denen die Ventilatorschaufeln einseitig befestigt angeordnet sind und wobei die Ventilatorschaufeln mit den Kränzen verbunden sind und in korrespondierende Kanäle auf der jeweils gegenüberliegenden Rotorenscheibe durchgreifen, die einen Materialdurchgang unter den Ventitatorschaufeh verhindern. Durch diese erfindungsgemäßen Maßnahmen wird eine wesentlich effizientere Mikronisierung erreicht unter gleichzeitiger Schonung der Vorrichtung selbst als sie im Stand der Technik bisher bekannt war. Erreicht wird dies dadurch, dass durch die Kanäle die Abnutzung der Ventilatorschaufeln selbst minimiert wird, indem bewusst ein Verbleiben von mikronisiertem Material innerhalb der Kanäle in Kauf genommen wird, was wiederum zu einem erhöhten Widerstand an den Ventilatorschaufeln selbst führt und damit letztlich zu einem erhöhten Grad der Mikronisierung.This object is achieved by the features listed in claim 1 and 2, namely, that micronized zeolites are used with a particle size diameter of less than 0.5 microns as filter cloth, which consist of rotors consisting of discs on which the fan blades on one side are arranged and wherein the fan blades are connected to the rings and pass through in corresponding channels on the respective opposite rotor disc, which prevent a passage of material under the Ventitatorschaufeh. By these measures according to the invention a much more efficient micronization is achieved while protecting the device itself as it was previously known in the art. This is achieved by minimizing the wear of the fan blades themselves by deliberately maintaining micronized material within the channels, which in turn leads to increased resistance on the fan blades themselves and, ultimately, to an increased degree micronization.

Die Vorteile der Zerkleinerung lassen sich wie folgt darstellen:

  • ■ Diese Feinmahlung wird durch kontrollierte Luftströmungen erzielt, die durch die Anwendung von neuartig konstruierten Ventilatorschaufeln hervorgerufen werden.
  • ■ Die Kanäle, in welchen die Ventilatorschaufeln durchgreifen, bilden ein geschlossenes Labyrinthsystem für die Materialverarbeitung, welches die Bewegung des Materials, das der Verarbeitung unterzogen ist, so kontrolliert, dass die Körnchen nicht ohne Schlag- und Reibungswirkung neben den Ventilatorschaufeln unverarbeitet vorbeifliegen, womit die Effizienz der Verarbeitung optimiert wird.
  • ■ Die zu erzielende Mikronisierung liegt bei 98,72 % aller Teilchen unter 4,3 µ. Ein Anteil von 28,36 % aller Teilchen weist sogar einen Durchmesser von unter 0,5 µm auf. Mit keinem herkömmlichen Verfahren oder einer bekannten Vorrichtung konnten derartige Ergebnisse erzielt werden.
The advantages of comminution can be represented as follows:
  • ■ This fine grinding is achieved through controlled airflow caused by the use of newly designed fan blades.
  • ■ The channels in which the fan blades pass through form a closed material processing labyrinth system which controls the movement of the material undergoing processing so that the granules do not pass unashamedly past the fan blades without impact and friction Efficiency of processing is optimized.
  • ■ The micronization to be achieved is 98.72% of all particles below 4.3 μ. A proportion of 28.36% of all particles even has a diameter of less than 0.5 microns. Such results could not be obtained by any conventional method or apparatus.

Das durch die erfindungsgemäße Vorrichtung mikronisierte Material weist vielerlei Vorteile für unterschiedlichste Verwendungsmöglichkeiten auf:The material micronized by the device according to the invention has many advantages for a wide variety of uses:

Die neuartige Vorrichtung ruft bei mineralischen Rohstoffkomponenten diverse chemische und chemisch-physikalische Veränderungen hervor. Die Effekte, welche durch dynamische Reibungsprozesse entstehen, verleihen diesen Mineralen neue Eigenschaften, die sich bei der Herstellung diverser Produkte technologisch und kommerziell nutzen lassen.The novel device causes diverse chemical and chemical-physical changes in mineral raw material components. The effects created by dynamic friction processes give these minerals new properties that can be used technologically and commercially in the manufacture of diverse products.

Aus der Gruppe der Zeolithe hat sich das Mineral Heulandit/Klinoptylolith aufgrund seiner Eigenschaften als vorteilhaft herausgestellt, nämlich aufgrund seiner Fähigkeit zur Wasseraufnahme, seiner Selektivität und lonenaustauschkapazität, sowie seiner chemischen Zusammensetzung, welche zeigte, daß dieses Mineral für den menschlichen Genuß absolut unbedenklich ist. Die mineralogischen und chemischen Eigenschaften von Klinoptilolithen wurden untersucht und stellen sich wie folgt dar: Tabelle 1 Komponente Anteil [%] von bis SiO2 61,96 67,17 TiO2 0,15 0,32 Al2O3 12,46 15,12 Fe2O 0,98 2,05 MnO spur 0,05 MgO 1,30 1,96 CaO 3,03 4,35 Na2O 0.70 1,11 K2O 0,78 1,32 H2O bei 100°C 4,05 4,74 H2O bei 1000°C 7,56 9,56 From the group of zeolites, the mineral heulandite / clinoptylolite has been found advantageous by virtue of its properties, namely its ability to absorb water, its selectivity and ion exchange capacity, and its chemical composition, which has shown that this mineral is absolutely harmless to human consumption. The mineralogical and chemical properties of clinoptilolites have been investigated and are as follows: <u> Table 1 </ u> component Proportion of [%] from to SiO 2 61.96 67.17 TiO 2 0.15 0.32 Al 2 O 3 12.46 15,12 Fe 2 O 0.98 2.05 MnO track 0.05 MgO 1.30 1.96 CaO 3.03 4.35 Na 2 O 0.70 1.11 K 2 O 0.78 1.32 H 2 O at 100 ° C 4.05 4.74 H 2 O at 1000 ° C 7.56 9.56

Der Kalziumgehalt dieses Minerals deutet darauf hin, daß es sich dabei um ein Kalziumzeolith handelt, welches in einer tuffartigen Struktur gebildet ist, d. h. es handelt sich hier um eine Art des Minerals Klinoptilolith mit den Eigenschaften der Heulanditgruppe. Das gemessene Raumgewicht des untersuchten Minerals Klinoptiloithes bewegt sich in dem Bereich von 1,41 bis 1,43 g/cm3. Difraktometrische und thermo-gravimetrische Untersuchungen zeigten, daß in allen untersuchten Mustern ungefähr gleicher Zeolithgehalt besteht. Die Ergebnisse der Röntgenuntersuchungen zeigen die Anwesenheit von folgenden Mineralsorten: Heulandithe (Klinoptilolithe), sowie in weiterer Folge im wesentlichen Quarz, Sand, Plagioklass und in einer geringen Menge auch Biothythe. Die mikroskopische Untersuchung mittels Elektronenmikroskop zeigte, daß die Materialstruktur aus feinen Tuffkömern besteht, welche eine homogene Isotropmasse, praktisch die Zeolithmaterie, darstellt. Der Gehalt dieser Materie bewegt sich grundsätzlich immer im Rahmen zwischen 70 % bis 85 %. Es ist in weiterer Folge die Anwesenheit von eckigen Quarzsegmenten festgestellt worden, sowie plagioklasse Sandkörner, welche in der Regel eine durchschnittliche Korngröße von 60 µm aufweisen. Die Untersuchung des Schmelzpunktes an 10 Mustern hat gezeigt, daß Klinoptilolithe bei einer Temperatur von 1260 - 1280° C schmelzen. Die festgestellte Härte laut Moss beträgt 3 - 3,5. Der Glühverlust beträgt: Tabelle 2 Glühverlust [Gew.-%] H2O bei 100 °C 3,34 bis 3,36 H2O bei 300 °C 5,42 bis 5,51 H2O bei 500 °C 2,60 bis 2,64 H2O bei 1000 °C 2,50 bis 2,51 Insgesamt 13,86 bis 13,92 The calcium content of this mineral indicates that it is a calcium zeolite formed in a tuff-like structure, ie, it is a kind of the mineral clinoptilolite having the properties of the heulandite group. The measured volume weight of the studied mineral clinoptiloite ranges from 1.41 to 1.43 g / cm 3 . Difractometric and thermo-gravimetric studies showed that approximately the same zeolite content exists in all the samples studied. The results of the X-ray studies show the presence of the following types of minerals: heulandithe (clinoptilolites), and subsequently essentially quartz, sand, plagioclase and, in a small amount, also biothythe. Microscopic examination by electron microscope showed that the material structure consists of fine tuff grains, which is a homogeneous isotropic mass, practically the zeolite matter. The content of this matter always moves in the range between 70% to 85%. It has subsequently been found the presence of angular quartz segments, as well as plagioclassic grains of sand, which generally have an average particle size of 60 microns. Examination of the melting point on 10 samples has shown that clinoptilolites melt at a temperature of 1260-1280 ° C. The determined hardness according to Moss is 3 - 3.5. The loss on ignition is: <u> Table 2 </ u> Loss on ignition [wt .-%] H 2 O at 100 ° C 3.34 to 3.36 H 2 O at 300 ° C 5.42 to 5.51 H 2 O at 500 ° C 2.60 to 2.64 H 2 O at 1000 ° C 2.50 to 2.51 All in all 13.86 to 13.92

Ergebnisse der Absorbtionsuntersuchungen: Tabelle 3 Zeitraum Wasser [Gew.-%] Benzol [Gew.-%] [h] von bis von bis 1 4,61 4,62 7,64 7,65 2 8.74 8,75 9,33 9,33 3 10,75 10,77 9,45 9,47 4 11,10 11,11 9,51 9,54 17 13,44 13,45 9,54 9,54 Results of absorption studies: <u> Table 3 </ u> Period Water [% by weight] Benzene [% by weight] [H] from to from to 1 4.61 4.62 7.64 7.65 2 8.74 8.75 9.33 9.33 3 10.75 10.77 9.45 9.47 4 11.10 11.11 9.51 9.54 17 13.44 13,45 9.54 9.54

Weitere Eigenschaften des untersuchten Klinoptilolithes: 1. Druckfestigkeit a)bei trockenem Zustand max. 426 kg/cm3 min. 361 kg/cm3 mittel 391 kg/cm3 b) mit Wasser gesättigten Zustand max. 360 kg/cm3 min. 253 kg/ cm3 mittel 292 kg/cm3 2. Wasseraufnahme 23,35 Gew.-% 3. Raumgewicht 1,37 g/cm3 Further properties of the examined clinoptilolite: 1. compressive strength a) when dry Max. 426 kg / cm 3 minute 361 kg / cm 3 mean 391 kg / cm 3 b) saturated with water Max. 360 kg / cm 3 minute 253 kg / cm 3 average 292 kg / cm 3 2. Water absorption 23.35% by weight 3. Volumetric weight 1.37 g / cm 3

Die Untersuchungsergebnisse der elektrischen Leitfähigkeit zeigten, daß die erfindungsgemäß behandelten Zeolithe bedeutend mehr Wasserstoffionen zu binden vermögen als die unbehandelten Zeolithe. Dies ist die unmittelbare Folge der Unterschiede in der Kristallstruktur der untersuchten Zeolithe, die durch die Feinmahlenung und Mikronisierung zustandegekommen sind. Die folgende Tabelle zeigt Beispiele für die Messungen der Leitfähigkeit und des pH der Suspension bei nicht behandelten und behandelten Zeolithen: Tabelle 4 Mischzeit der Suspension a Konzentration an Zeolith (mg/ml H2O) pHb (unaktiviertes Zeolith) pHb (erfindungsgemäß behandeltes Zeolith) Leitfähigkeitc (unaktiviertes Zeolith) µS/cm Leitfähigkeitc (erfindungsgemäß behandeltes Zeolith) µS/cm 2 Std. 20 7,35 7,48 157 147 2 Std. 40 6,45 7,22 198 180 2 Std. 60 6,81 7,35 307 280 20 Std. 40 6,67 6,90 259 218 20 Std. 80 6,96 7,40 48 Std. 80 6,87 7,44 a mit Magnetrührer, 70 - 100 RPM;
b pH Messung unmittelbar nach der Zentrifugation (15 Minuten auf 7000 RPM),
c Leitfähigkeitsmessung im Überstand unmittelbar nach der Zentrifugation (15 Minuten auf 7000 RPM), Leitfähigkeit des redestillierten Wassers beträgt 1.8 µS/cm
The investigation results of the electrical conductivity showed that the zeolites treated according to the invention are able to bind significantly more hydrogen ions than the untreated zeolites. This is the direct consequence of the differences in the crystal structure of the investigated zeolites, which are the result of fine grinding and micronization. The following table shows examples of conductivity and pH measurements of the suspension in untreated and treated zeolites: <u> Table 4 </ u> Mixing time of the suspension a Concentration of zeolite (mg / ml H 2 O) pH b (unactivated zeolite) pH b (zeolite treated according to the invention) Conductivity c (unactivated zeolite) μS / cm Conductivity c (zeolite treated according to the invention) μS / cm 2 hours. 20 7.35 7.48 157 147 2 hours. 40 6.45 7.22 198 180 2 hours. 60 6.81 7.35 307 280 20 hours 40 6.67 6.90 259 218 20 hours 80 6.96 7.40 48 hours 80 6.87 7.44 a with magnetic stirrer, 70-100 RPM;
b pH measurement immediately after centrifugation (15 minutes at 7000 RPM),
c Conductivity measurement in the supernatant immediately after centrifugation (15 minutes at 7000 RPM), conductivity of the redistilled water is 1.8 μS / cm

Die Ergebnis ist, daß der pH-Wert der unbehandelten zu den behandelten Zeolithe steigt, während die Leitfähigkeit abnimmt. Das erfindungsgemäß behandelte Material zeigt überraschende Wirkungen im Hinblick auf die Minimierung gesundheitsschädlicher Inhaltsstoffe von Filterzigaretten.The result is that the pH of the untreated to the treated zeolites increases while the conductivity decreases. The material treated according to the invention shows surprising effects with regard to the minimization of harmful components of filter cigarettes.

Zigarettenrauch ist ein sichtbares, verdunstendes Produkt der Tabakverbrennung, der Additive und des Zigarettenpapiers, der gleich nach der Verbrennungszone entsteht und sich wie folgt zusammensetzt:

  • ■ gasförmige Phase (CO, CO2, O2, H2, N2N-Oxyd, HCN, HCNS, NH3, Aldehyde, Alkohole usw.),
  • ■ starr-flüssige Phase, zusammengesetzt aus Wasser und in ihr ganz oder teilweise schmelzende Verbindungen (wie Nikotin und weitere Alkaloide), die während des Rauchens destillieren, verdunsten oder verbrennen.
Cigarette smoke is a visible, evaporating product of tobacco combustion, additives and cigarette paper, which is produced immediately after the combustion zone and is composed as follows:
  • ■ gaseous phase (CO, CO 2 , O 2 , H 2 , N 2 N-oxide, HCN, HCNS, NH 3 , aldehydes, alcohols, etc.),
  • ■ rigid-liquid phase, composed of water and all or part of its melting compounds (such as nicotine and other alkaloids) that distill, evaporate or burn during smoking.

Während der Rauch durch den Tabak zieht, kommt es zur Abkühlung und Kondensation, ein Teil des Rauches gelangt in die Mundhöhle. Wegen der Verringerung der möglichen negativen, gesundheitsschädlichen Folgen des Rauches wird bekanntermaßen als Mundstück der Zigarette ein Zigarettenfilter eingebaut.As the smoke runs through the tobacco, it cools and condenses, and some of the smoke gets into the oral cavity. Because of the reduction of the possible negative, unhealthy consequences of the smoke is known to be installed as a mouthpiece of the cigarette, a cigarette filter.

Der klassische Filter ist der Zellulose-Acetat-Filter. Um die Effizienz des Filters zu vergrößern (Fähigkeit des Zurückhaltens, der Absorption starrflüssiger und gasförmiger Phasen des Rauches), werden Additive, wie es Aktivkohle, Zeolithe, Silikagel, Magnesiumsilikat und künstliches Hämoglobin sind, verwendet.The classic filter is the cellulose acetate filter. In order to increase the efficiency of the filter (ability of retention, absorption of the liquid and gaseous phases of the smoke), additives such as activated carbon, zeolites, silica gel, magnesium silicate and artificial hemoglobin are used.

Bekannt sind Mehrfachfilter, Papierfilter, Kombinationen mehrerer Filter und Additiva. Die Effizienz zur Reduzierung schädlicher Komponenten eines einfachen (Zellulose-Acetat-) Filters beträgt 20 - 65 %; durch verschiedene neuartig entwickelte Kombinationen, Additiva und Formen der Filter wird die Effizienz auf ca. 75 % angehoben. Ein großer Marktanteil kommt heute schon den sogenannten Leicht-Zigaretten ("Lights" oder "Ultra") zu, die weniger Trockenrauch-Kondensat, Wasser, Nikotin, CO2 und andere schädliche Komponenten enthalten oder verursachen. Beim Projektieren von Light-Zigaretten nutzt man die Ventilation am Filter (Verdünnung des Rauches), verlängertes Wickelpapier der Filter (skirt tipping) und eine Kombination verschiedener Zigarettenpapiere und verschiedener Tabake. Die Effizienz und die Selektierung des Filters (erhöhte Fähigkeit der Absorption bestimmter Komponenten), sind ein wichtiger Faktor beim Projektieren der Light-Zigaretten. Einer der wichtigen Faktoren bei der Konstruktion des Filters und auch der Zigarette, ist der Saugwiderstand (pressure drop), der wesentlich auf den Geschmack und die Leichtigkeit des Rauchens Einfluß hat. Viele Additive und Konstruktionslösungen vergrößern den Saugwiderstand und ungewollte Effekte beim Rauchen. Dies ist der einfache Grund, warum noch immer beim größten Teil die einfachen Zellulose-Acetat-Filter verwendet werden.Are known multiple filters, paper filters, combinations of multiple filters and Additiva. Efficiency to reduce harmful components of a simple (cellulose acetate) filter is 20-65%; through various newly developed combinations, additives and forms of filters, the efficiency is raised to about 75%. Today, a large market share already goes to the so-called light cigarettes ("lights" or "ultra"), which contain or cause less dry smoke condensate, water, nicotine, CO 2 and other harmful components. When designing light cigarettes use the ventilation on the filter (thinning of the smoke), extended paper wrap of the filter (skirt tipping) and a combination of different cigarette papers and different tobaccos. The efficiency and the selection of the filter (increased ability of absorption of certain components), are an important factor when designing the light cigarettes. One of the important factors in the design of the filter and also the cigarette, the pressure drop, which has a significant influence on the taste and the ease of smoking. Many additives and design solutions increase the suction resistance and unwanted effects during smoking. This is the simple reason why most of the simple cellulose acetate filters are still used.

Das erfindungsgemäß behandelte Material erhöht überraschenderweise die Effizienz und Selektion der Filter, sowie ein Anhalten und eine Verbesserung des gewünschten Geschmackes der Zigarette; dabei wird der Saugwiderstand des Filters kaum verändert. Die behandelten Zeolithe weisen eine größere Absorptionstärke auf, was auf die Veränderungen im Kristallgitter zurückzuführen ist.The material treated according to the invention surprisingly increases the efficiency and selection of the filters, as well as stopping and improving the desired taste of the cigarette; while the suction resistance of the filter is hardly changed. The treated zeolites have a larger Absorption strength, which is due to the changes in the crystal lattice.

Vorteilhaft hat sich ein Filterzusatz bei Zellulose-Acetat Filtern als Pulver mit einer Korngöße von 0,2 bis 0,5 µm erwiesen.Advantageously, a filter additive in cellulose acetate filters has proven to be a powder with a particle size of 0.2 to 0.5 microns.

Bei der Herstellung der Filter, kann man die erfindungsgemäß behandelten Zeolithe direkt auf die Zellulose-Acetat-Faser oder das Papier bzw. Crest aufbringen - wie einen Zusatz im Hohlraum eines Multifilters, kombiniert mit dem Dualfilter usw.In the preparation of the filter, one can apply the zeolites treated according to the invention directly to the cellulose acetate fiber or the paper or crest - such as an additive in the cavity of a multifilter, combined with the dual filter, etc.

Filter, die Gegenstand eines kontrollierten Experiments waren, wurden durch Hinzufügen von erfindungsgemäß behandelten Zeolithen direkt auf die Zellulose-Acetat-Faser produziert, nachdem man Plastifikatoren (Triacetin) vor dem Formen der Filterstäbchen im Zylinder eingesetzt hat. Das Pulver wurde durch ein besonders ausgearbeitetes Dosimeter direkt auf die Faser aufgebracht. Dadurch war es möglich, fast einheitlich bis zu 70 mg des erfindungsgemäß behandelten Zeoliths pro Filterstäbchen hinzuzufügen. Diese Art der Zugabe des Pulvers beeinflußt die Arbeit der herkömmlichen Maschinen und das Formen der Filterstäbchen nicht wesentlich, da die Maschinen zur Herstellung der Füterstäbchen einen dafür vorgesehenen Raum im Arbeitsfluß für diese Applikation haben. Durch diese Art der Zugabe des Pulvers ändert sich die Technologie der Stäbchenproduktion nicht wesentlich. Das technologische Verfahren wird nur um den Preis der Additive erhöht.Filters that were the subject of a controlled experiment were produced by adding zeolites treated according to the invention directly to the cellulose acetate fiber after using plasticizers (triacetin) prior to forming the filter rods in the cylinder. The powder was applied directly to the fiber through a specially designed dosimeter. This made it possible to add almost uniformly up to 70 mg of the zeolite treated according to the invention per filter rod. This way of adding the powder does not significantly affect the work of the conventional machines and the forming of the filter sticks, since the machines for making the sticks have a dedicated space in the working flow for this application. By this way of adding the powder, the technology of rod production does not change significantly. The technological process is only increased by the price of the additives.

Die durchschnittlichen Resultate der gemessenen physischen Filterparameter ohne Zusatz von erfindungsgemäß behandelten Zeolithen und mit Zusatz von erfindungsgemäß behandelten Zeolithen, werden nachfolgend dargestellt. Tabelle 5 Muster Saugwiderstand Filtermasse Zugabe von erfindungsgemäß behandelten Zeolith [mm VS] [mg] 12 cm Filter 2 cm Filter 0 390 721 0 0 1 392 750 3,0 0,50 2 395 765 5,0 0,83 3 395 766 7,6 1,27 4 410 773 10,0 1,66 5 440 782 68,0 11,30 The average results of the measured physical filter parameters without the addition of zeolites treated according to the invention and with the addition of zeolites treated according to the invention are shown below. <u> Table 5 </ u> template suction resistance filter mass Addition of zeolite treated according to the invention [mm VS] [Mg] 12 cm filter 2 cm filter 0 390 721 0 0 1 392 750 3.0 0.50 2 395 765 5.0 0.83 3 395 766 7.6 1.27 4 410 773 10.0 1.66 5 440 782 68.0 11,30

Die Zugabe der Zeolithe hat sich nicht wesentlich auf den Saugwiderstand und auch nicht auf das Gewicht des 12 cm langen Filterstäbchens ausgewirkt.The addition of the zeolites did not significantly affect the wicking resistance nor the weight of the 12 cm long filter stick.

Die erhaltenen Resultate sind Durchschnitte der Messungen von 500 Filterstäbchen von jedem Muster. Der Anteil des zugegebenen behandelten Zeoliths wurde aufgrund des Unterschiedes der erhaltenen Menge Asche beim Verbrennen der Filterstäbchen im Mufon-Ofen bei 525° C berechnet. Für die Verarbeitung der Zigarette wurde im wesentlichen herkömmliches Filterpapier ohne Ventilation und ein Tabakgemisch, welches bei der Herstellung von full flavour-Zigaretten des Typs American Blend verwendet wird. Die verarbeiteten Zigaretten wurden nach Gewicht und Saugwiderstand sortiert und auf der Rauchmaschine (Borgwaldt RM 20) nach dem ISO-Standard erprobt. Jedes Muster wurde 5 mal auf der Maschine erprobt. Die Menge an Trockenrauch-Kondensat (Total Particule Matter), Nikotin, CO2, Wasser und Teer wurden bestimmt. Alle Analysen wurden nach dem geltenden ISO-Standard; die Menge an Nikotin im Trockenrauch-Kondensat durch Extraktion mit 2-Propanol und anschließender HPLC durchgeführt.The results obtained are averages of the measurements of 500 filter rods from each sample. The proportion of the treated zeolite added was calculated from 525 ° C due to the difference in the amount of ash obtained when burning the filter sticks in the Mufon oven. For the processing of the cigarette was substantially conventional filter paper without ventilation and a mixture of tobacco, which is used in the production of full flavor American Blend cigarettes. The processed cigarettes were sorted by weight and suction resistance and tested on the smoking machine (Borgwaldt RM 20) according to the ISO standard. Each sample was tested 5 times on the machine. The amount of Total Particulate Matter, nicotine, CO 2 , water and tar were determined. All analyzes were performed according to the current ISO standard; the amount of nicotine in the dry smoke condensate was carried out by extraction with 2-propanol and subsequent HPLC.

Die erhaltenen durchschnittlichen Resultate sind in der nachfolgenden Tabelle dargestellt, aus der ersichtlich ist, dass bei Erhöhung des zugegebenen erfindungsgemäß behandelten Zeoliths im Filter, sich der Anteil an Nikotin, Trockenrauch-Kondensat, Teer, Wasser und CO2 im Hauptstrom des Zigarettenrauches verringert. Gesetzlich sind die Zigarettenhersteller verpflichtet, den Gehalt an Teer und Nikotin in der Zigarette anzugeben. Dies macht die Bedeutung der Wesensart des CO2 nicht geringer, welches negative Einwirkungen auf den Respiratorzyklus des Organismus hat. Das erfindungsgemäß behandelte Zeolith beseitigt überraschenderweise offenbar selektiv die schädlichen Komponente im Hauptstrom des Zigarettenrauches. Unabhängig von der Menge des Zeoliths, das auf den Filter appliziert wurde, ändert sich der Widerstand der Zigarette nicht wesentlich, aber auch nicht die Verbrennungsgeschwindigkeit. Die Leichtigkeit und Annehmlichkeit des Rauchens wurde beibehalten. Die Degustationsprüfungen haben gezeigt, dass die Muster mit dem größten Anteil an dem erfindungsgemäß behandelten Zeolith (Muster 5 - 11,3 mg und Muster 4 -1,66 mg) einen verbesserten Rauchgeschmack haben und ein hervorgehobenes Aroma aufweisen, so dass sie allgemein angenehmer zu rauchen sind. Tabelle 6 Muster Zusammensetzung Einheit 0 1 2 3 4 5 Erfindungsgemäß behandeltes Zeolith Filter [mg] 0 0,50 0,83 1,27 1,66 11,30 Trockenrauch-Kondensat Zigarette [mg] 14,8 14,2 13,5 13,2 12,9 10,8 Nikotin Zigarette [mg] 1,03 0,98 0,94 0,93 0,91 0,75 CO2 Zigarette [mg] 14,98 14,37 13,61 12,46 11,86 10,90 Wasser Zigarette [mg] 1,18 1,05 1,09 0,95 0,73 0,68 Teer Zigarette [mg] 12,6 12,2 11,5 11,3 11,3 9,4 Tabakmasse in Zigarette [mg] 764 759 770 787 752 764 Anzahl der Züge Züge/Zigarette 7,4 7,0 7,4 7,5 7,2 7,4 Saugwiderstand der Zigarette [mm VS] 102 102 105 109 108 111 The average results obtained are shown in the table below, from which it can be seen that as the added zeolite treated in the filter increases, the level of nicotine, dry smoke condensate, tar, water and CO 2 in the main stream of cigarette smoke decreases. Legally, cigarette manufacturers are required to indicate the content of tar and nicotine in the cigarette. This does not diminish the importance of the nature of CO 2 , which has negative effects on the respiratory cycle of the organism. Surprisingly, the zeolite treated according to the invention apparently selectively removes the harmful component in the main stream of cigarette smoke. Regardless of the amount of zeolite applied to the filter, the resistance of the cigarette does not change significantly, nor does it change the burning rate. The ease and convenience of smoking has been maintained. The tasting tests have shown that the samples with the largest proportion of the zeolite treated according to the invention (samples 5 - 11.3 mg and sample 4 - 1.66 mg) have an improved smoky taste and a pronounced aroma, so that they are generally more agreeable are smoking. <u> Table 6 </ u> template composition unit 0 1 2 3 4 5 Treated zeolite according to the invention Filter [mg] 0 0.50 0.83 1.27 1.66 11,30 Dry smoke condensate Cigarette [mg] 14.8 14.2 13.5 13.2 12.9 10.8 nicotine Cigarette [mg] 1.03 0.98 0.94 0.93 0.91 0.75 CO 2 Cigarette [mg] 14.98 14,37 13.61 12.46 11.86 10,90 water Cigarette [mg] 1.18 1.05 1.09 0.95 0.73 0.68 tar Cigarette [mg] 12.6 12.2 11.5 11.3 11.3 9.4 Tobacco mass in cigarette [Mg] 764 759 770 787 752 764 Number of trains Trains / cigarette 7.4 7.0 7.4 7.5 7.2 7.4 Suction resistance of the cigarette [mm VS] 102 102 105 109 108 111

In der nachfolgenden Tabelle sind die gemessenen durchschnittlichen Werte der Filter nach dem Rauchen dargestellt. Die Menge an Trockenrauch-Kondensat wurde aus dem Differenz der Menge des Produktionsmaterials vor und nach dem Rauchen berechnet. Die Menge des Nikotins wurde durch Extraktion aus dem Filter in 2-Propanol und Wasser durch die Karl-Fisher Methode bestimmt. Die Resultate zeigen, dass die mit dem erfindungsgemäß behandelten Zeolith applizierten Filter, eine erhöhte Fähigkeit der Absorption von Trockenrauch-Kondensat, Nikotin, und Wasser haben, welches die vorangegangenen Messungen und Resultate unterstreicht. Tabelle 7 Muster Zusammensetzung Einheit 0 1 2 3 4 5 Erfindungsgemäß behandeltes Zeolith mg/Filter 0,00 0,50 0,83 1,27 1,66 11,30 Trockenrauch-Kondensat mg/Filter 13,50 13,30 13,80 14,30 14,80 15,40 Nikotin mg/Filter 0,53 0,58 0,60 0,60 0,67 0,69 Wasser mg/Filter] 1,01 1,02 1,03 1,12 1,05 1,12 The following table shows the measured average values of the filters after smoking. The amount of dry smoke condensate was calculated from the difference in the amount of production material before and after smoking. The amount of nicotine was determined by extraction from the filter in 2-propanol and water by the Karl-Fisher method. The results show that the filters applied with the zeolite treated according to the invention have an increased ability to absorb of dry smoke condensate, nicotine, and water, which underlines the previous measurements and results. <u> Table 7 </ u> template composition unit 0 1 2 3 4 5 Treated zeolite according to the invention mg / Filter 0.00 0.50 0.83 1.27 1.66 11,30 Dry smoke condensate mg / Filter 13.50 13,30 13.80 14,30 14,80 15.40 nicotine mg / Filter 0.53 0.58 0.60 0.60 0.67 0.69 water mg / filter] 1.01 1.02 1.03 1.12 1.05 1.12

Aus diesen Ergebnissen folgt, dass eine Beimengung des erfindungsgemäß behandelten Minerals von 0,5 mg (vgl. Muster 1) vorteilhaft ist, da der Anteil an Trockenrauch-Kondensat abnimmt. Auch geht aus dieser Tabelle hervor, dass ein verstärktes Zurückhalten von Nikotin im Filter zu beobachten ist.From these results, it follows that an admixture of the mineral treated according to the invention of 0.5 mg (see sample 1) is advantageous, since the proportion of dry smoke condensate decreases. It is also clear from this table that there is an increased retention of nicotine in the filter.

Durch die Applikation des erfindungsgemäß behandelten Zeoliths auf Zellulose-Acetat-Faser von Zigarettenfiltern führt also zu einer verstärkten Retention schädlicher Komponenten des Hauptstromes des Zigarettenrauches, zufriedenstellenden physischen Eigenschaften, ohne aber negativen Einfluß auf die degustativen und Raucheigenschaften einer Zigarette zu bewirken. Der Zusatz von 0,50 mg des erfindungsgemäß behandelten Zeoliths pro Filter beseitigt 4 % Trockenrauch-Kondensat, CO2 und Nikotin, sowie 11 % Wasser. Ein Zusatz von 11,30 mg vom erfindungsgemäß behandelten Zeoliths pro Filter beseitigt 27 % Trockenrauch-Kondensat, CO2 und Nikotin, sowie 42 % Wasser aus dem Hauptstrom des Rauches.The application of the zeolite treated according to the invention to cellulose acetate fiber of cigarette filters thus leads to an increased retention of harmful components of the main stream of the cigarette smoke, satisfactory physical properties, but without having a negative effect on the degustative and smoking properties of a cigarette. The addition of 0.50 mg of the zeolite treated per filter according to the invention eliminates 4% dry smoke condensate, CO 2 and nicotine, and 11% water. An addition of 11.30 mg of zeolite per filter treated according to the invention eliminates 27% dry smoke condensate, CO 2 and nicotine, and 42% water from the main stream of smoke.

Ferner ist vorteilhaft eine weitere Zugabe von Selen (bis 25 µg/Filter) zu dem erfindungsgemäß behandelten Zeolith, da dadurch die Absorption freier Radikale, die durch Verbrennungen entstehen, erhöht wird.Furthermore, a further addition of selenium (up to 25 .mu.g / filter) to the zeolite treated according to the invention is advantageous since it increases the absorption of free radicals which are formed by burns.

Eine Vorrichtung, welche zur Zerkleinerung des Zeoliths verwendet wird und zu den vorteilhaften Eigenschaften des zerkleinerten Materials führt, wird nachfolgend beschrieben. Es zeigt:

Figur 1
eine schematische Ansicht der erfindungsgemäßen Vorrichtung;
Figur 2
einen vertikalen Schnitt durch die Vorrichtung;
Figur 3
eine Rotorenscheibe;
Figur 3a
einen vertikalen Schnitt durch einen Ausschnitt der zusammengesetzten Vorrichtung,
Figur 3b
eine Ausschnittvergrößerung entlang eines Schnittes A-A gemäß der Fig. 3a;
Figur 4
die schematische Andeutung der Luftströme entlang der Ventilatorschaufeln;
Figur 5
die schematische Andeutung des zerkleinerten Materials entlang der Ventilatorschaufeln;
Figur 6
eine Ventilatorschaufel mit Stift/Kanal im Detail und in mehreren Ansichten (6a, 6b, 6c);
Figur 7
schematische Darstellung einer Segmenten-Ventilatorschaufel;
Figur 7a
Ausschnitt entlang eines Schnittes A-A gemäß Figur 7.
A device which is used for comminuting the zeolite and leading to the advantageous properties of the comminuted material is described below. It shows:
FIG. 1
a schematic view of the device according to the invention;
FIG. 2
a vertical section through the device;
FIG. 3
a rotor disk;
FIG. 3a
a vertical section through a section of the composite device,
FIG. 3b
a detail enlargement along a section AA according to FIG. 3a;
FIG. 4
the schematic indication of the air flows along the fan blades;
FIG. 5
the schematic indication of the crushed material along the fan blades;
FIG. 6
a fan blade with pin / channel in detail and in several views (6a, 6b, 6c);
FIG. 7
schematic representation of a segment fan blade;
Figure 7a
Section along a section AA according to FIG. 7.

Die Figur 1 zeigt eine Vorrichtung 10 für die Feinmahlung und Mikronisierung, sowie das Homogenisieren von diversen festen und flüssigen Rohstoffkomponenten. Das Prinzip sieht derart aus, dass das Ausgangsmaterial durch die Mitte der Rotoren in den Verarbeitungsraum der Vorrichtung eingesaugt wird. Der Eintritt wird durch die Einwirkung von zentrifugalen Kräften in den Raum zwischen den Ventilatorschaufeln begünstigt und wird aufgrund der dort herrschenden Luftströme beschleunigt; so dass das Material mit dem bereits verarbeiteten Material kollidiert. Das Ausgangsmaterial wechselt die Bewegungsrichtung in sehr kurzen Intervallen; infolgedessen wird es zerkleinert und mikronisiert.1 shows a device 10 for the fine grinding and micronization, and the homogenization of various solid and liquid raw material components. The principle is such that the starting material is sucked through the center of the rotors into the processing space of the device. The entry is favored by the action of centrifugal forces in the space between the fan blades and is accelerated due to the prevailing air currents there; so that the material collides with the already processed material. The source material changes direction of movement in very short intervals; As a result, it is crushed and micronized.

Die Vorrichtung 10 besteht aus einem aufklappbaren Gehäuse 11 mit einem Materialeinfuhrschacht 11d, in welchem sich zwei Rotorenscheiben 12 befinden, die gegeneinander gestellt sind und mittels entsprechender Motoren 13 über Riemen 13a gegenläufig betrieben werden, so dass sie sich mit gleicher Winkelgeschwindigkeit drehen. Das Gehäuse 11 und die Motoren 13 sind auf dem Fundament 14 befestigt und bilden eine unabhängige Einheit.The device 10 consists of a hinged housing 11 with a Materialeinfuhrschacht 11d, in which there are two rotor discs 12, which are opposed to each other and operated by respective motors 13 via belt 13a in opposite directions, so that they rotate at the same angular velocity. The housing 11 and the motors 13 are mounted on the foundation 14 and form an independent unit.

Figur 2 zeigt, dass das Gehäuse 11 aus zwei Teilen aufgebaut ist: eine Gehäuseseite 11 a für die Materialeinfuhr und eine weitere Gehäuseseite 11b mit Einfuhrschacht 11c. Diese zwei Seiten 11a, 11b sind miteinander verschraubt. Auf beiden Seiten des Gehäuses 11 befinden sich die Träger 15, in welche die Lager 16 und Reckstangen 17 eingebaut sind. Auf der Seite 11a für die Materialeinfuhr befindet sich ein Rohr 18 für die geregelte Einfuhr des Materials; auf der unteren Seite befindet sich eine Öffnung 19 für den Ausstoß des fertigen Materials.Figure 2 shows that the housing 11 is constructed of two parts: a housing side 11 a for the material import and a further housing side 11 b with insertion shaft 11 c. These two sides 11a, 11b are bolted together. On both sides of the housing 11 are the carrier 15, in which the bearings 16 and stretch rods 17 are installed. On the side 11a for the material import is a pipe 18 for the controlled import of the material; on the lower side there is an opening 19 for the discharge of the finished material.

Figur 3, 4 und 5 zeigt, dass auf den Rotorenscheiben 12 mehrere konzentrische Kränze 20 mit den Stiften 21 und Ventilatorschaufeln 22 angeordnet sind, welche so konstruiert und ausgerichtet sind, dass sie berührungsfrei, während sie gegenläufig drehen, nebeneinander vorbeilaufen können - angedeutet durch die Drehrichtung 25. Minimal sind zwei Kränze erforderlich, die von den zwei Rotoren angetrieben werden. Die Aufgabe der Schlagstifte 21. und der Ventilatorschaufeln 22 ist die Erzeugung von turbulenten Luftströmungen für die Beschleunigung des verarbeiteten Materials, so dass Stöße und Reibung unter den Körnchen bei bestimmten Winkeln unter dynamischen Bedingungen hervorrufen werden. Die Kanäle 23 auf den Scheiben verhindern den Materialdurchgang unter den Ventilatorschaufeln 22, vgl. Figur 3 a und 3b.Figures 3, 4 and 5 show that on the rotor disks 12 a plurality of concentric rings 20 are arranged with the pins 21 and fan blades 22, which are constructed and oriented so that they can run past each other without contact as they rotate in opposite directions - indicated by the Turning 25. Minimum two wreaths are required which are driven by the two rotors. The task of the striker pins 21 and fan blades 22 is to create turbulent airflows for the acceleration of the processed material so that shocks and friction among the granules at certain angles will create dynamic conditions. The channels 23 on the discs prevent the passage of material under the fan blades 22, see. Figure 3 a and 3b.

Das Ausgangsgranulat (nicht dargestellt) wird, durch den Zentralteil 18 des Motorensystems durch Einsaugung eingebracht, durch die Luftströme 26 beschleunigt und so gesteuert, dass die Körnchen infolge mehrmaliger Bewegungsrichtung untereinander kollidieren und sich in sehr kurzen Zeitintervallen aneinander reiben. Dabei berühren sich die Arbeitswerkzeuge und andere Teile der Vorrichtung nicht oder nur geringfügig - aber es kommt auf keinen Fall zu Zerstörungen der Werkzeuge. Es entsteht eine Interaktion unter den Körnchen mit solchem Ausmaß, dass bei den Körnchen die innere Energie ausgetauscht wird, da die Zusammenstöße unplastisch sind (vgl. Fig. 4 und 5).The starting granules (not shown), introduced by the central portion 18 of the engine system by suction, accelerated by the air streams 26 and controlled so that the grains collide with each other due to repeated movement direction and rub against each other in very short time intervals. The tools and other parts of the device do not touch or only slightly - but it comes in no case to destruction of the tools. An interaction occurs among the granules to such an extent that in the granules the internal energy is exchanged since the collisions are aplastic (see Figures 4 and 5).

Die Effekte, die Folge der Zusammenstöße der Körnchen sowie Folge der relativen Bewegung der Oberfläche eines Körnchen über der Oberfläche von einem anderen Körnchen (mechanische Reibung) sind, werden verstärkt durch diejenigen Effekte, die infolge plötzlicher Richtungswechsel der Kömchenbewegung entstehen, so dass die Energie der Beschleunigung und relativer Bewegung der Körnchen in Energie der Deformierung, sowie in die Energie der molekularen Bewegung umgewandelt wird. Während der Zusammenstöße und der Reibung der Körnchen, welche dem Verkleinerungsprozeß in sehr kurzen Zeitintervallen (10-5 bis 10-6 s) unterzogen sind, entsteht eine bedeutende Veränderung ihrer Geometrie bzw. Form und Größe. Durch die relative Bewegung eines Körnchens über der Oberfläche eines anderen Körnchens, entstehen Schäden und Deformierungen der Körnchenoberfläche, sowie der Materialschichten, welche sich unmittelbar unter der Kornoberfläche befinden. Dadurch wird die Struktur des Kristallgitters auf der Oberfläche zerstört oder geschädigt, so dass teilweise die Kristallform in eine amorphe Phase umgewandelt wird, mit dem Ergebnis, dass die physikalischen und physikalisch-chemischen, sowie energetischen Eigenschaften des verarbeitenden Materials verändert werden. Bei solchen Verarbeitungen von Rohstoffkomponenten organischen Ursprungs zerreißen beispielsweise Zellulosefasern und große Molekülen werden mithin zu kleineren Molekülen, wobei diverse Veränderungen chemischer Zusammensetzung bei dem verarbeiteten Material hervorgerufen werden, sowie auch physikalische Veränderungen, die bedeutend für ihre weitere Materialverarbeitungen und/oder Aufbereitung, aber auch für die Wirksamkeit sind.The effects resulting from the collisions of the granules as well as the relative movement of the surface of one granule over the surface of another granule (mechanical friction) are exacerbated by those effects which result from sudden changes of direction of the granular motion, so that the energy of the granules Acceleration and relative movement of grains is transformed into energy of deformation, as well as into the energy of molecular motion. During the collisions and the friction of the granules, which are subjected to the reduction process in very short time intervals (10 -5 to 10 -6 s), a significant change in their geometry or shape and size arises. The relative movement of a grain over the surface of another grain causes damage and deformation of the granule surface, as well as the layers of material that lie just below the grain surface are located. This destroys or damages the structure of the crystal lattice on the surface, thus partially transforming the crystal form into an amorphous phase, with the result that the physical and physicochemical and energetic properties of the processing material are altered. For example, in such processing of raw material components of organic origin, cellulose fibers and large molecules break down into smaller molecules, causing various changes in chemical composition of the material being processed, as well as physical changes important for their further material processing and / or processing, but also for the effectiveness are.

Neben der Veränderung der Eigenschaften des Materials, welches mit den beschriebenen Verfahren verarbeitet wird, wird dieses infolge von mechanischen Beanspruchungen fein gemahlen und mikronisiert und die Veränderung der granulometrischen Zusammensetzung des Materials ist von der Granulometrie der Ausgangskörner, sowie vom Niveau der Kömchenbeschleunigung, der geplanten Winkel der Zusammenstöße und gegenseitigen Reibung, sowie die geplanten Anzahl der Zusammenstöße abhängig. Folgende Parameter für die Feinmahlung und Mikronisierung mit der erfindungsgemäßen Vorrichtung stellen eine optimale Konfiguration dar, so dass diese Parameter bevorzugt sind:

  • ■ Granulation des Ausgangskoms < 4,0 mm
  • ■ Anzahl der Gesamtzahl der Kränze/Kranzreihen auf den Rotorenscheiben: 5
  • ■ Durchmesser der Rotoren 500 mm
  • ■ Drehzahl der Rotoren 3600 /Min.
  • ■ Kapazität der Vorrichtung 300Kg/Std.
In addition to changing the properties of the material, which is processed by the described method, this is finely ground and micronized due to mechanical stresses and the change in the granulometric composition of the material is the granulometry of the starting grains, as well as the level of Kömchenbeschleunigung, the planned angle the collisions and mutual friction, as well as the planned number of collisions dependent. The following parameters for the fine grinding and micronization with the device according to the invention represent an optimal configuration, so that these parameters are preferred:
  • ■ Granulation of the exit area <4.0 mm
  • ■ Number of total wreaths / crown rows on the rotor discs: 5
  • ■ Diameter of the rotors 500 mm
  • ■ Rotor speed 3600 / min.
  • ■ Device capacity 300Kg / hr.

Verglichen mit den Materialien, welche auf herkömmliche technische Weise (vgl. DE 197 55 921.2 ) feingemahlen und mikronisiert werden, zeigt das Material, welches durch die erfindungsgemäße Vorrichtung feingemahlen und mikronisiert wurde, eine erhöhte freie Energie und Reaktionsfähigkeit.Compared with the materials which in a conventional technical manner (see. DE 197 55 921.2 ) and micronized, the material which has been finely ground and micronized by the device according to the invention shows increased free energy and reactivity.

Die Innovation liegt mithin in der Konstruktion (Form, Verzahnung, Neigung) und Austauschbarkeit von Stiften und Ventilatorschaufeln auf die konstruierten Kanäle, die sich auf der Rotorenscheibe befinden, sowie in der Auswahl des Materials für die Ausarbeitung von Ventilatorschaufeln. Die Rotationsscheiben der Vorrichtung rotieren mit der gleichen Winkelgeschwindigkeit, bewegen sich jedoch gegenläufig. Das Ausgangsmaterial wird durch das Einsaugrohr 18 in den Zentralteil der rotierenden Scheibe eingeführt, aufgrund von Zentrifugalkräften werden die Körnchen der Rohstoffkomponente in Richtung des äußeren Randes des Gehäuses beschleunigt. Die Körnchen schlagen auf die Kränze 20 der Ventilatorschaufeln 22, welche sich in Gegenrichtung drehen. Sie wechseln die Bewegungsrichtung aufgrund der Richtungswechsel der Ventilatorschaufeln. Ferner schlagen und reiben sich die Körnchen untereinander, gehen nachfolgend in einen weiteren Kranz 20 mit Ventilatorschaufeln 22 über, wechseln wieder die Richtung der Bewegung im Einklang mit dem Richtungswechsel der rotierenden Scheibe, solange bis sie das Schaufelsystem verlassen. Am Ende der Bearbeitung in der erfindungsgemäßen Vorrichtung schlagen die Körnchen auf der Wand des Gehäuses auf und werden durch die Ausgangsöffnung 19 abtransportiert.The innovation is therefore in the design (shape, toothing, inclination) and interchangeability of pins and fan blades on the constructed channels, which are located on the rotor disc, as well as in the selection of material for the development of fan blades. The rotation discs of the device rotate at the same angular velocity, but move in opposite directions. The raw material is introduced into the central portion of the rotating disk through the suction pipe 18, and due to centrifugal forces, the granules of the raw material component are accelerated toward the outer periphery of the casing. The granules strike the rims 20 of the fan blades 22, which rotate in the opposite direction. They change the direction of movement due to the change of direction of the fan blades. Further, the grains beat and rub one against the other, then proceeding into another ring 20 with fan blades 22, again changing the direction of movement in accordance with the directional change of the rotating disk until they leave the paddle system. At the end of processing in the device according to the invention, the granules strike the wall of the housing and are transported away through the outlet opening 19.

Figur 3a und 3b zeigt, dass die Kanäle 23 auf den Scheiben 12, in welche die Ventilatorschaufeln 22 durchgreifen, den Materialdurchgang unter den Ventilatorschaufeln 22 verhindern. Deren Form wird gemäß den Eigenschaften der jeweils zu verarbeitenden Rohstoffkomponenten (Materials) - also Granulation des Ausgangsmaterials, seine Feuchtigkeit, Härte, Ursprung, chemische Zusammensetzung und ähnliches - definiert. Wenn z. B. die Eingangsgranulation des Materials < 1 mm beträgt, bedeutet dies, dass der minimale Abstand zwischen den Ventilatorschaufeln und den Kanälen auf den Scheiben größer als 1 mm sein soll, um überhaupt das Durchgehen des Materials zu ermöglichen. Bei der Ausarbeitung und der Montage der Scheiben soll zufriedenstellende Parallelität verwirklicht werden, um den Ventilatorschaufeln das Durchgreifen in die Kanäle zu ermöglichen, denn die Durchmesser der Scheiben sind relativ groß (500 mm). Vorteile gegenüber der in der DE 197 55 921.1 beschriebenen Vorrichtung liegen darin, dass die Ventilatorschaufeln aufgrund ihrer Form, Neigung und Verzahnung bei dem Prozeß der Feinmahlung und Mikronisierung mit einer feinen Schicht des verarbeiteten Materials belegt werden und auf diese Weise von der Schlag- und Reibungswirkung des Eingangsmaterials geschützt werden. Die Abnutzung der Oberfläche der Ventilatorschaufeln wird somit minimiert und die Lebensdauer bedeutend verlängert. Ferner wird die energetische Ladung des Materials, welches behandelt wird, angehoben, wenn die Körnchen untereinander kollidieren und nicht mit den Teilen der Ventilatorschaufeln. Die technologischen Parameter, wie die Anzahl der Ventilatorschaufeln, ihre Neigung, die Form der Schaufelverzahnung, Anzahl der Ventilatorkränze, Winkelgeschwindigkeit der Scheiben, definieren die späteren Eigenschaften des verarbeiteten Materials. Mit der Kombination der angeführten Parameter wird es möglich, die Ergebnisse und Effekte zu programmieren.FIGS. 3a and 3b show that the channels 23 on the disks 12, in which the fan blades 22 pass, prevent the material passage under the fan blades 22. Their shape is defined according to the properties of the respective raw material components (material) to be processed - ie granulation of the starting material, its moisture, hardness, origin, chemical composition and the like. If z. For example, if the input granulation of the material is <1 mm, this means that the minimum distance between the fan blades and the channels on the Slices should be greater than 1 mm, to allow even the passage of the material. During the preparation and assembly of the panes, satisfactory parallelism should be achieved in order to allow the fan blades to penetrate into the channels, because the diameters of the panes are relatively large (500 mm). Advantages over in the DE 197 55 921.1 described device are that the fan blades are occupied due to their shape, inclination and toothing in the process of fine grinding and micronization with a fine layer of the processed material and are protected in this way from the impact and friction effect of the input material. The wear of the surface of the fan blades is thus minimized and the life extended significantly. Further, the energetic charge of the material being treated is raised when the granules collide with each other and not with the parts of the fan blades. The technological parameters, such as the number of fan blades, their inclination, the shape of the blade teeth, number of fan crowns, angular velocity of the discs, define the later properties of the processed material. By combining the mentioned parameters it becomes possible to program the results and effects.

In der Figur 3b sind weiter Scheibenkanäle (23) näher dargestellt. In den Rotorenscheiben (12) befinden sich an denjenigen Orten, die mit der Kranzreihe (20) des gegenüberliegenden Rotors (13) korrespondieren, Ausnehmungen (20a; siehe Fig. 3a, 3b), innerhalb derer die Ventilatorschaufeln (22) des gegenüberliegenden Kranzes (20) laufen. Die Kanäle (23) decken sich gegenseitig mit der Länge a, welche 2 - 5 mm beträgt. Sie bilden quasi ein Labyrinth, welches den Durchgang des Materials unter den Ventilatorschaufeln verhindert. Durch die Entstehung des Labyrinthes verstärkt sich der Widerstand für die Strömung unter den Ventilatorschaufeln. Somit wird erreicht, dass sich die Körnchen des Ausgangsmaterials durch die Hauptströmung zwischen den Ventilatorschaufeln bewegen. Die Form der Kanäle wird gemäß technisch-technologischer Eigenschaften der Rohstoffkomponenten des verarbeiteten Materials definiert (Granulation des Ausgangsmaterials, seine Feuchtigkeit, Härte, Ursprung, chemische Zusammensetzung und ähnliches). Wenn es die Scheibenkanäle nicht geben würde, würde sich das Ausgangsmaterial aufgrund der Zentrifugalkräfte so bewegen, dass es vom Zentrum bis zu der Peripherie der Scheiben an den Ventilatorschaufeln und der Scheibe vorbeigeht. Bei der Ausgangsgranulation des Materials von 0 - 1 mm muß die Entfernung zwischen den Ventilatorschaufeln und den Kanälen größer als 1 mm sein, um den Durchgang des Materials überhaupt zu ermöglichen, vorteilhaft hat sich eine Entfernung von 2 mm genauso wie für die Verdeckung a erwiesen.In the figure 3b further disc channels (23) are shown in more detail. In the rotor disks (12), recesses (20a, see Figures 3a, 3b) are located at those locations corresponding to the row of corrugations (20) of the opposite rotor (13), within which the fan blades (22) of the opposite ring (20). 20). The channels (23) cover each other with the length a, which is 2 - 5 mm. They form a kind of labyrinth, which prevents the passage of the material under the fan blades. The emergence of the labyrinth increases resistance to the flow under the fan blades. Thus, it is achieved that the granules of the starting material move through the main flow between the fan blades. The shape of the channels is in accordance with technical-technological characteristics of the raw material components of processed material (granulation of the starting material, its moisture, hardness, origin, chemical composition and the like). If there were not the disc channels, the source material would move due to the centrifugal forces passing from the center to the periphery of the discs on the fan blades and disc. At the initial granulation of the material of 0-1 mm, the distance between the fan blades and the channels must be greater than 1 mm to allow passage of the material at all, advantageously a distance of 2 mm has proven to be the same as for the occlusion a.

Die Figuren 6, 6a, 6b und 6c zeigen die Geometrie der Ventilatorschaufeln 22 und der Stifte 21. Der Kranz 20, die Ventilatorschaufeln 22 und die Stifte 21 sind aus Hartstahl gebaut. Eine Alternative ist, den Stift aus Porzellan und die Ventilatorschaufeln aus Stahl herzustellen. Die Neigung der Ventilatorschaufeln 22 beträgt im Verhältnis zur Horizontalen α = 4 - 15° mit der Optimierung auf 8 - 10°. Die Anordnung und die Größe von der Verzahnung ist von der Anzahl der Ventilatorschaufeln abhängig (β = 30 - 120° und γ = 60 - 120°). Der Biegungsgrad der Ventilatorschaufeln ist mit dem Verhältnis der Längen a und b definiert, wobei b 10 % der Sehnenlänge darstellt. Die Anordnung der Ventilatorschaufeln ist fixiert. Sie sind in die Kranzform in entsprechende Ausnehmungen eingepreßt Die Form der Ventilatorschaufeln, profilierte Kollisionsoberfläche 22a, 22b und die Neigung sichern die Abfüllung der Ventilatorschaufeln mit dem Ausgangsmaterial und werden damit von der Abnutzungswirkung des Ausgangsmaterials geschützt, was auf die Verlängerung der Lebensdauer der Ventilatorschaufeln wirkt. Die Zähne 22b auf den Ventilatorschaufeln halten die erste Schicht des Ausgangsmaterials auf der Kollisionsoberfläche 22a, während die zweite Schicht langsam über die erste Schicht rutscht und diese zweite Schicht nimmt die Schläge des ankommenden Ausgangsmaterials an. Bevor die Ventilatorschaufeln 22 in die jeweilige Kranzreihe 20 der Rotorenscheibe 12 eingebracht wird, wird der Stift 21 in die Rotorenscheibe 12 eingepreßt. Die Symmetrieachse des Stiftes 21 befindet sich in der Symmetrieachse des Biegungsgrades der Ventilatorschaufeln 22, damit die Geometrie des Systems der Ventilatorschaufeln/Stifte optimal erreicht wird. Während der Materialverarbeitung schlagen die Materialkörnchen auf die Stirnseite der Ventilatorschaufeln und insbesondere auf und in die Stifte. Der Stift wird somit abgenutzt. Nach der Abnutzung wird der Stift durch Auspressen oder Bohren durch einen neuen ausgetauscht. Dies hat einen entscheidenden Vorteil: Bisherige Varianten der Ventilatorschaufeln ohne Stifte haben die Abnutzung der Ventilatorschaufeln selbst ergeben. Der Austausch der abgenutzten Ventilatorschaufeln ist im Vergleich mit dem Austausch der Stifte sehr kompliziert, aufwendig und teuer. Die Stifte können daher leicht ausgetauscht werden; die Ventilatorschaufeln bleiben unbeschädigt und müssen es nicht. De Austausch der Ventilatorschaufein erfolgt erst bei allgemeiner Materialermüdung.Figures 6, 6a, 6b and 6c show the geometry of the fan blades 22 and the pins 21. The rim 20, the fan blades 22 and the pins 21 are made of high carbon steel. An alternative is to make the porcelain pin and the fan blades made of steel. The inclination of the fan blades 22 is in relation to the horizontal α = 4 - 15 ° with the optimization to 8 - 10 °. The arrangement and the size of the toothing depends on the number of fan blades (β = 30 - 120 ° and γ = 60 - 120 °). The degree of flexing of the fan blades is defined by the ratio of lengths a and b, where b represents 10% of the chord length. The arrangement of the fan blades is fixed. The shape of the fan blades, profiled collision surface 22a, 22b and the incline secure the filling of the fan blades with the starting material and are thus protected from the wear effect of the starting material, which acts to extend the life of the fan blades. The teeth 22b on the fan blades hold the first layer of starting material on the collision surface 22a while the second layer slowly slips over the first layer and this second layer accepts the impacts of the incoming source material. Before the fan blades 22 are introduced into the respective rim row 20 of the rotor disk 12, the pin 21 is pressed into the rotor disk 12. The symmetry axis of the pen 21 is located in the axis of symmetry of the degree of bending of the fan blades 22, so that the geometry of the system of fan blades / pins is optimally achieved. During material processing, the granules strike the end face of the fan blades, and in particular onto and into the pins. The pen is thus worn. After wear, the pin is replaced by pressing or drilling through a new one. This has a decisive advantage: Previous variants of the fan blades without pins have resulted in the wear of the fan blades themselves. The replacement of the worn fan blades is very complicated compared to the replacement of the pins, consuming and expensive. The pins can therefore be easily replaced; The fan blades are undamaged and do not have to. The replacement of the fan blade only takes place during general material fatigue.

Das Problem der Vibrationen und der Festigkeit der Stifte ist dadurch gelöst, dass sich der Stift 21 mit der Fläche von 1/3 seines. Stiftumfanges an eine korrespondierende Ausnehmung der Ventilatorschaufel 22 an diese Ventilatorschaufeln "anlehnt", und sich nicht geradflächig an die Ventilatorschaufeln anlehnt. Die Ventilatorschaufeln 22 werden durch Kaltpressen verformt oder auch durch Schmieden, wobei das Schmieden der besseren Aushärtung dient.The problem of the vibrations and the strength of the pins is solved in that the pin 21 with the area of 1/3 of his. Stiftumfanges to a corresponding recess of the fan blade 22 to these fan blades "leans", and does not lean against the fan blades on a straight surface. The fan blades 22 are deformed by cold pressing or by forging, whereby the forging serves for better curing.

Eine andere Ausführungsform sieht erfindungsgemäß auch Segment-Ventilatorschaufeln (Figur 7, 7a) vor. Die Segment-Ventilatorschaufeln 22 werden aus Keramik oder Gußstahl hergestellt. Bei dieser Ausführungsform werden in die Rotorenscheiben 12 die Kanäle eingebaut, in welche die Segment-Ventilatorschaufeln mit unbestimmten Einlegungen gestellt werden. Die Genauigkeit der Einstellungen und die Festigkeit der Ventilatorschaufeln wird durch das Profil der Kanäle und durch die Reibung zwischen den Segment-Ventilatorschaufeln und die tragende Scheibe bestimmt. Die Neigung der Ventilatorschaufeln in Bezug auf die Horizontale beträgt α = 4 - 15° mit der Optimierung bei 8° - 10°. Die Einordnung der Zähne 22b und ihre Größe ist von der Länge der Ventilatorschaufeln 22 abhängig, Winkel β beträgt 30° - 120°, und Winkel γ beträgt 60° - 120°. Der Biegungsgrad der Ventilatorschaufeln ist mit dem Verhältnis der Längen a und b definiert, wobei b 10 % der Sehnenlänge darstellt. Die Form der Ventilatorschaufeln, der profilierten (verzahnten) Kollisionsoberfläche und der Neigung sichern, dass die Ventilatorschaufeln mit dem Ausgangsmaterial abgefüllt werden und damit von der Abnutzungswirkung des Ausgangsmaterials geschützt werden, was auf die Verlängerung der Lebensdauer der Ventilatorschaufeln wirkt. Die Zähne 22b auf den Ventilatorschaufeln halten wie in Figur 6 die erste Schicht des Ausgangsmaterials auf der Kollisionsoberfläche 22a, während die zweite Schicht langsam über die erste Schicht rutscht und diese zweite Schicht nimmt die Schläge des ankommenden Ausgangsmaterials an. Diese Ausführung hat im Vergleich zu obiger Ausführung (Fig. 6) den Vorteil, dass die Ventilatorschaufeln mit verschiedenen Neigungen (Winkel α) eingebaut werden können; somit ist der Austausch der Ventilatorschaufeln einfacher. Die Form der Ventilatorschaufeln hat keine Aussparung für die Stifte.Another embodiment according to the invention also provides segment fan blades (FIGS. 7, 7a). The segment fan blades 22 are made of ceramic or cast steel. In this embodiment, the channels are incorporated into the rotor discs 12, in which the segment fan blades are placed with indefinite deposits. The accuracy of the settings and the strength of the fan blades is determined by the profile of the channels and by the friction between the segment fan blades and the supporting disc. The inclination of the fan blades with respect to the horizontal is α = 4 - 15 ° with the optimization at 8 ° - 10 °. The classification of the teeth 22b and their size is Depending on the length of the fan blades 22, angle β is 30 ° - 120 °, and angle γ is 60 ° - 120 °. The degree of flexing of the fan blades is defined by the ratio of lengths a and b, where b represents 10% of the chord length. The shape of the fan blades, the profiled (toothed) collision surface and the slope ensure that the fan blades are filled with the source material and thus protected from the wear effect of the source material, which acts to extend the life of the fan blades. The teeth 22b on the fan blades, as in FIG. 6, hold the first layer of the starting material on the collision surface 22a, while the second layer slowly slips over the first layer, and this second layer absorbs the impacts of the incoming source material. This embodiment has the advantage over the previous embodiment (Figure 6) that the fan blades can be installed with different inclinations (angle α); Thus, the replacement of the fan blades is easier. The shape of the fan blades has no recess for the pins.

Bezugszeichenreference numeral

1010
Vorrichtungcontraption
1111
Gehäusecasing
11a11a
Gehäuseseite zur MaterialeinfuhrHousing side for material import
11b11b
Gehäuseseite mit VerschlußdeckelHousing side with cap
11c11c
Verschlußdeckelcap
11d11d
MaterialeinfuhrschachtMaterial insertion slot
1212
Rotorenscheibenrotors disks
1313
MotorenEngines
13a13a
Riemenbelt
1414
Fundament / GestellFoundation / frame
1515
Trägercarrier
1616
Lagercamp
1717
ReckstangenHorizontal bars
1818
Einfuhrrohrimport pipe
1919
Auslaßoutlet
2020
Kränzewreaths
20a20a
Ausnehmungrecess
2121
Stiftepencils
2222
Ventilatorschaufelnfan blades
22a22a
Kollisionsflächecollision surface
22b22b
Verzahnunggearing
2323
Kanälechannels
2424
Zermahlenes MaterialCrushed material
2525
Drehrichtungdirection of rotation
2626
Luftströmeairflows

Claims (5)

  1. Use of micronized zeolites as filter additives in filtration processes, the grain diameter of said micronized zeolites being below 0.5 µm, characterized in that the zeolites used have been reduced in size by means of impellers constituted of disks having the ventilator blades arranged thereon, mounted on one side, said ventilator blades being connected with the rims, extending into corresponding channels on each opposing impeller disk, which prevent passage of material beneath the ventilator blades.
  2. Use of micronized zeolites as filter additives in filter cigarettes, characterized in that the grain diameter of the micronized zeolites is below 0.5 µm, particularly between 0.2 µm and 0.5 µm, which zeolites have been reduced in size by means of impellers constituted of disks having the ventilator blades arranged thereon, mounted on one side, said ventilator blades being connected with the rims, extending into corresponding channels on each opposing impeller disk, which prevent passage of material beneath the ventilator blades.
  3. The use according to claim 2, characterized in that the micronized zeolites are directly applied to the cellulose acetate fiber of the filter or to the paper or Crest.
  4. The use according to claim 3, characterized in that up to 11.3 mg of micronized zeolites per filter, preferably 0.5 mg per filter, are employed.
  5. The use according to at least one of claims 2 to 4, characterized in that selenium is added at a concentration of up to 25 µg per filter.
EP02090411A 1999-04-26 1999-04-26 Use of micronised zeolites as filter material Expired - Lifetime EP1317886B1 (en)

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SI9930982T SI1317886T1 (en) 1999-04-26 1999-04-26 Use of micronised zeolites as filter material
DE59914387T DE59914387D1 (en) 1999-04-26 1999-04-26 Use of micronized zeolites as filter materials

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EP99913546A EP1107826A1 (en) 1999-04-26 1999-04-26 Device for micronizing materials
PCT/IB1999/000757 WO2000064586A1 (en) 1999-04-26 1999-04-26 Device for micronizing materials

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EP02090410A Revoked EP1316530B1 (en) 1999-04-26 1999-04-26 Micronised zeolites for use as pharmaceutical agents
EP02090409A Withdrawn EP1316255A1 (en) 1999-04-26 1999-04-26 Use of micronized minerals as plant protection agent
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EP99913546A Withdrawn EP1107826A1 (en) 1999-04-26 1999-04-26 Device for micronizing materials

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DK (1) DK1316530T3 (en)
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PT1316530E (en) 2005-04-29
ATE365002T1 (en) 2007-07-15
EP1316255A1 (en) 2003-06-04
ES2234981T3 (en) 2005-07-01
EP1316530A1 (en) 2003-06-04
EP1316530B1 (en) 2004-12-15
EP1317886A1 (en) 2003-06-11
SI1316530T1 (en) 2005-06-30
HRP990263A2 (en) 2009-04-30
ATE284840T1 (en) 2005-01-15
DK1316530T3 (en) 2005-04-25
AU3164899A (en) 2000-11-10
WO2000064586A1 (en) 2000-11-02
EP1107826A1 (en) 2001-06-20
ES2289051T3 (en) 2008-02-01

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